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Production technology of nitroguanidine

A production process and technology for nitroguanidine, applied in the field of nitroguanidine production technology, can solve the problems of large amount of waste acid and low content of crude nitroguanidine, and achieve the effect of no three wastes

Active Publication Date: 2013-02-13
NANTONG TENDENCI CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there are 1-2 large-scale production enterprises in China producing nitroguanidine, but the content of crude nitroguanidine prepared is low, about 90%, the yield is only 86%, and the amount of waste acid is relatively large

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Add 1000Kg concentrated sulfuric acid into a 2000-liter enamel reaction kettle, stir the solution at a speed of 68-69r / min, the reaction kettle is jacketed, and -10°C cooling brine is passed inside, and the content of 90% is slowly added to the reaction kettle 500Kg of guanidine nitrate, the feed rate of guanidine nitrate is based on the temperature of the reaction solution being controlled between 30-40°C. After the feeding is completed, the dehydration reaction is carried out at 39-41°C for 1 hour, and the dehydration reaction ends;

[0014] Add 4000 liters of water into the hydrolysis reaction kettle, control the water temperature between 5-10°C, stir at a speed of 68-69r / min, then add the above dehydration reaction solution, the addition speed of the dehydration reaction solution is to control the temperature of the hydrolyzate not to exceed 30 ℃ as the benchmark, after the addition is completed, the hydrolysis reaction is carried out at a temperature of 20-30 ℃ for ...

Embodiment 2

[0017] The steps described in Example 1, the difference is that the quality of concentrated sulfuric acid is 1100Kg, and the final obtained hydrous nitroguanidine crude product has a loss on drying: 26% (water), content: 97.9% (HPLC), weight: 514 Kg, molar yield: 97.1%.

Embodiment 3

[0019] Describe the steps with Example 1, the difference is that the volume of water added in the hydrolysis reactor is 3000 liters, and finally obtain the crude product of hydrous nitroguanidine, its loss on drying: 25% (water), content: 97.5% (HPLC), Weight: 513 Kg, molar yield: 97.8%.

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PUM

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Abstract

The invention discloses a production technology of nitroguanidine. The nitroguanidine serves as a raw material, a nitroguanidine crude product is obtained after sulfuric acid dehydration, ice water hydrolysis and liquid ammonia neutral reaction, and ammonium sulfate in filtrate is recycled through multiple-effect evaporation. The technology has the advantages that the prepared nitroguanidine has a molar yield higher than 95% and a content larger than 97%, and three wastes seldom exist.

Description

technical field [0001] The invention relates to a production process of nitroguanidine. Background technique [0002] Nitroguanidine, the molecular formula is C(NH 2 ) 2 NNO 2 , is white crystal, easily soluble in hot water and lye, slightly soluble in ethanol and dilute sulfuric acid, insoluble in ether and cold water. As a raw material for organic synthesis, it is used as an intermediate for imidacloprid and acetamiprid in pesticides, and is used as a raw material for the synthesis of N-nitroiminoimidazolidine, an intermediate in the next step. In addition, aminoguanidine can be produced after reduction, which can be used for the synthesis of angina pectoris drug Lekoan, etc. It can also be used for the preparation of nitrocellulose gunpowder, nitroglycerin gunpowder and the admixture of diethylene glycol dinitrate, and an important component of solid rocket propellant. [0003] At present, there are 1-2 large-scale production enterprises in China producing nitroguanid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C279/34C07C277/08
Inventor 周甦谭建平金标
Owner NANTONG TENDENCI CHEM
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